CN104689789A - TiO2/activated carbon fiber nano-composite photocatalysis film and preparation method and application thereof - Google Patents

TiO2/activated carbon fiber nano-composite photocatalysis film and preparation method and application thereof Download PDF

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Publication number
CN104689789A
CN104689789A CN201510130664.4A CN201510130664A CN104689789A CN 104689789 A CN104689789 A CN 104689789A CN 201510130664 A CN201510130664 A CN 201510130664A CN 104689789 A CN104689789 A CN 104689789A
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nacf
tio
film
solution
carbon fiber
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Inventor
麦立强
王柄量
郭一川
杨子洲
田蜜蜜
刘晓威
王瑜
贾舒然
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a TiO2/activated carbon fiber nano-composite photocatalysis film and a preparation method and application thereof. The method comprises the steps that 1, activated carbon fiber is washed through deionized water, soaked into a nitric acid solution and dried after being washed; 2, the processed activated carbon fiber obtained in the step 1 is cut into pieces of the appropriate size, and the pieces are connected with the negative electrode of a power source; the positive electrode of the power source is connected with a platinum electrode, the activated carbon fiber and the platinum electrode are soaked into a peroxo titanic acid solution to be fixed, and power-on treatment is carried out to obtain a TiO2/activated carbon fiber nano film precursor; 3, the TiO2/activated carbon fiber nano film precursor obtained in the step 2 is naturally dried to be placed into a vacuum tubular furnace, thermal treatment is carried out, cooling is performed naturally to reach the room temperature. The TiO2/activated carbon fiber nano-composite photocatalysis film has the advantage that poisonous and harmful gas can be rapidly degraded through the synergistic effect of the TiO2 and the activated carbon fiber.

Description

TiO 2/ NACF nano composite photocatalytic film and its preparation method and application
Technical field
The invention belongs to new material and energy-conserving and environment-protective field, particularly relate to a kind of TiO 2/ NACF nano composite photocatalytic film and its preparation method and application.
Technical background
TiO 2be a kind of important functional material, its anatase crystal structure can produce great activity under the irradiation of ultraviolet light, can degradable organic pollutant, pernicious gas, air solid small particles etc.Due to above reason, TiO 2be widely used in the fields such as water, air and environmental improvement.Therefore, TiO 2film increases its photo-catalysis capability because the photocatalysis performance of its excellence is loaded on multiple substrate.At present, various substrate is studied both at home and abroad, and by TiO 2film is carried on the surface of the materials such as pottery, metal, glass, graphite.
ACF (NACF) efficiently absorption property and adsorption and desorption speed fast, easy regeneration, acidproof, alkaline-resisting, there are good electric conductivity and chemical stability etc., be widely used in the aspects such as water treatment, household and finishing, environment-friendly engineering and medical and health.The NACF produced in China mainly contains following several: phenolic aldehyde base fiber, PAN base fiber, sticky glue based fibre, pitch-based fiber.
Prior art did not also openly report TiO 2/ NACF nano composite photocatalytic film and preparation method thereof.
Summary of the invention
Technical problem to be solved by this invention provides a kind of TiO for above-mentioned prior art 2/ NACF nano composite photocatalytic film and preparation method thereof, realizes bi-material compound by electrochemical method, simple and easy to do, possesses and prepares potentiality on a large scale.
The present invention solves the problems of the technologies described above adopted technical scheme: TiO 2/ NACF nano composite photocatalytic film, it is that on NACF, load has TiO 2film, described TiO 2the thickness of film is 10 ~ 100nm, is following preparation method's products therefrom, comprises the following steps:
1) deionized water detergent active Carbon fibe, soaks 18 ~ 36h in salpeter solution, after again washing, dries by deionized water;
2) by step 1) NACF is cut into suitable size after the process that obtains, be connected with power cathode; Positive source is connected with platinum electrode, NACF and platinum electrode is together immersed in peroxo titanic acid sol fixing, and energising process 40min ~ 80min, obtains TiO 2/ NACF nano thin-film presoma;
3) by step 2) TiO that obtains 2be put in vacuum tube furnace after the natural drying of/NACF nano thin-film presoma, heat treatment 60 ~ 120min under the condition of 150 DEG C ~ 400 DEG C, is down to room temperature naturally.
By such scheme, the preparation method of described peroxo titanic acid sol is: according to volume ratio 1:4:(50 ~ 80) measure TiCl 4solution, H 2o 2and absolute ethyl alcohol, ice-water bath dropwise drips TiCl while stirring in absolute ethyl alcohol 4solution, after solution-stabilized, dropwise drips H in solution 2o 2, after stable, remove ice-water bath, stir 40min ~ 60min, ageing, obtains stable red colloidal sol.
By such scheme, step 1) NACF that uses is commercially available viscose-based active carbon fiber, specific area is 1300 ~ 1500m 2/ g.
By such scheme, step 2) in NACF and platinum electrode to keep at a distance 1cm ~ 5cm, supply voltage 3v ~ 10v, make to remain on 15-25mA/cm by the current density of NACF 2.
Described TiO 2the preparation method of/NACF nano composite photocatalytic film, comprises the following steps:
1) deionized water detergent active Carbon fibe, soaks 18 ~ 36h in salpeter solution, after again washing, dries by deionized water;
2) by step 1) NACF is cut into suitable size after the process that obtains, be connected with power cathode; Positive source is connected with platinum electrode, NACF and platinum electrode is together immersed in peroxo titanic acid sol fixing, and energising process 40min ~ 80min, obtains TiO 2/ NACF nano thin-film presoma;
3) by step 2) TiO that obtains 2be put in vacuum tube furnace after the natural drying of/NACF nano thin-film presoma, heat treatment 60 ~ 120min under the condition of 150 DEG C ~ 400 DEG C, is down to room temperature naturally.
Described TiO 2/ NACF nano composite photocatalytic film is as the application of photocatalytic degradation material.
Key reaction mechanism of the present invention: the present invention first carries out pretreatment to NACF, makes it surface and hangs with a large amount of oxy radical, strengthen itself and TiO 2attachment degree; Adopt TiCl 4sol method, prepares presoma peroxo titanic acid sol, makes it and the NACF strong bonded with oxy radical, after sintered, and TiO 2growth at NACF on the surface, thus successfully realizes fixing TiO 2.
Beneficial effect of the present invention: the present invention innovatively proposes TiO 2the combination of photochemical catalyst and sorbing material NACF, realizes bi-material compound by electrochemical method, simple and easy to do, possesses and prepares potentiality on a large scale; Pass through TiO 2with the synergy of NACF, realize the fast degradation to poisonous and hazardous organic gas.The NACF that the present invention adopts has extra specific surface area (1300-1500m 2/ g), can a large amount of dusty gas of rapid adsorption, thus enrichment dusty gas, effectively improve TiO 2surface unit area internal contamination gas concentration, passes through TiO 2light-catalyzed reaction, gained TiO of the present invention 2/ NACF nano composite photocatalytic film realizes the efficient degraded rapidly to pollutant.
Accompanying drawing explanation
Fig. 1 is the embodiment of the present invention 1 gained TiO 2the HRSEM figure of the single fiber of/NACF nano composite photocatalytic film;
Fig. 2 is the embodiment of the present invention 1 gained TiO 2the TiO of/NACF nano composite photocatalytic film 2the HRSEM figure of thicknesses of layers;
Fig. 3 is the TiO described in embodiment 1 2the EDS of/NACF nano composite photocatalytic film analyzes data.
Specific embodiments
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1:
TiO 2/ NACF nano composite photocatalytic material, adopts following electrochemical preparation method, comprises the following steps:
1) by deionized water, by ACF washing, (NACF used is commercially available viscose-based active carbon fiber, and specific area is 1300m 2/ g), immerse 24h in salpeter solution, after again washing by deionized water, put into 60 DEG C of oven for drying;
2) TiCl is got according to volume ratio 1:4:60 4solution, 30%H 2o 2, absolute ethyl alcohol, stir under ice-water bath condition, in absolute ethyl alcohol, dropwise drip TiCl 4solution.After solution-stabilized, in solution, dropwise drip 30%H 2o 2, be configured to 65ml colloidal sol and remove ice-water bath after stable, stir 40min ~ 60min, ageing 12h with rotating speed 500r/min;
3) in step 2) basis on, by step 1) ACF that obtains is cut into 2cm*2cm size, be connected with power cathode.Positive source links with platinum electrode, together immerses above-mentioned ACF and platinum electrode according to step 2) fixing in the colloidal sol prepared, keep NACF and platinum electrode distance 1cm, voltage 3v, make to remain on 20mA/cm by the current density of NACF 2, electrochemical treatments 40min;
4) in step 3) basis on, by step 3) be put in vacuum tube furnace after the ACF natural drying that obtains, heat treatment 100min under the condition of 400 DEG C, Temperature fall is to room temperature.
With product TiO of the present invention 2/ ACF photocatalysis film material is example, and its composition is determined by EDS (EnerDispersiveSpectroscopy, X-ray energy spectrometer).EDS shows, ACF surface distributed has Ti element, and content conforms to thickness (as shown in Figure 3), visible in figure, TiO 2successfully be coated on NACF surface.HRSEM test shows, TiO 2layer is evenly attached to ACF fiber surface, forms stratiform homogeneous film; Visible TiO in Fig. 2 2the even coated ACF fiber of layer, thin film layer thickness is about 40nm.
With the TiO of gained of the present invention 2/ NACF nano composite photocatalytic thin-film material is tested, and is to carry out in the light tight glass box of black that inwall is coated with one deck aluminium-foil paper, at room temperature carries out whole Degradation Formaldehyde test.Experimental procedure is as follows: the bottom first glass dish being placed with 2cm*2cm small pieces catalyst being placed on light tight glass box, and above glass dish, cover a sizable smooth glass sheet, then, the concentrated formaldehyde (mass fraction is 38%) of 10 μ L is injected into test box inside.In addition, in the process of whole reaction, power is the inside that the electric fan of 5W size is placed on test box always, and this comes to make the formaldehyde of injection spread rapidly.Through 1-2h, the formaldehyde of test box inside volatilizees completely, and its final concentration of formaldehyde tends towards stability, remains on about 170ppm.HCHO content in whole course of reaction to be connected with infrared photoacoustic spectroscopy (INNOVA Air Tech Instruments Model 1412) Real-Time Monitoring and obtaining by test box.Concentration of formaldehyde starts the test experience of Degradation Formaldehyde reach adsorption equilibrium in test box after.Within one hour, the bright degradation rate of Degradation Formaldehyde table with test results reaches 58.04%, proves that gained thin-film material photocatalytic degradation handling property of the present invention is excellent.
Embodiment 2:
TiO 2/ NACF nano composite photocatalytic material, adopts following electrochemical preparation method, comprises the following steps:
1) by deionized water, ACF is washed, immerse 24h in salpeter solution.After again washing by deionized water, put into 60 DEG C of oven for drying;
2) TiCl is got according to volume ratio 1:4:60 4solution, 30%H 2o 2, absolute ethyl alcohol, ice-water bath condition lower magnetic force stir, in absolute ethyl alcohol, dropwise drip TiCl 4solution.After solution-stabilized, in solution, dropwise drip 30%H 2o 2, be configured to 130ml colloidal sol.After stable, remove ice-water bath, stir 60min, ageing 12h with rotating speed 500r/min;
3) in step 2) basis on, by step 1) ACF that obtains is cut into 3cm*4cm, be connected with power cathode.Positive source links with platinum electrode, together immerses above-mentioned ACF and platinum electrode according to step 2) fixing in the colloidal sol prepared, keep NACF and platinum electrode distance 2cm, voltage 5v, make to remain on 25mA/cm by the current density of NACF 2, electrochemical treatments 40min;
4) in step 3) basis on, by step 3) be put in vacuum tube furnace after the ACF natural drying that obtains, heat treatment 100min under the condition of 350 DEG C, Temperature fall is to room temperature.
With the TiO of gained of the present invention 2/ ACF photocatalysis film material 3cm*4cm small pieces carry out Degradation Formaldehyde test in a hour, and test result is that one hour degradation rate reaches 77.09%, prove that gained thin-film material photocatalysis performance of the present invention is excellent.
Embodiment 3:
TiO 2/ NACF nano composite photocatalytic material, adopts following electrochemical preparation method, comprises the following steps:
1) by deionized water, ACF is washed, immerse 24h in salpeter solution.After again washing by deionized water, put into 60 DEG C of oven for drying;
2) TiCl is got according to volume ratio 1:4:60 4solution, 30%H 2o 2, absolute ethyl alcohol, ice-water bath condition lower magnetic force stir, in absolute ethyl alcohol, dropwise drip TiCl 4solution.After solution-stabilized, in solution, dropwise drip 30%H 2o 2, be configured to 65ml colloidal sol and remove ice-water bath after stable, stir 50min, ageing 12h with rotating speed 400r/min;
3) in step 2) basis on, by step 1) ACF that obtains is cut into 2cm*2cm, be connected with power cathode.Positive source links with platinum electrode, together immerses above-mentioned ACF and platinum electrode according to step 2) fixing in the colloidal sol prepared, keep NACF and platinum electrode distance 1cm, voltage 3v, make to remain on 15mA/cm by the current density of NACF 2, electrochemical treatments 60min;
4) in step 3) basis on, by step 3) be put in Muffle furnace after the ACF natural drying that obtains, heat treatment 100min under the condition of 200 DEG C, Temperature fall is to room temperature.
With the TiO of gained of the present invention 2/ ACF photocatalysis film material 2cm*2cm small pieces carry out Degradation Formaldehyde test in a hour, and test result one hour degradation rate reaches 60.47%, prove that gained thin-film material photocatalysis performance of the present invention is excellent.
Embodiment 4:
TiO 2/ NACF nano composite photocatalytic material, adopts following electrochemical preparation method, comprises the following steps:
1) by deionized water, ACF is washed, immerse 24h in salpeter solution.After again washing by deionized water, put into 60 DEG C of oven for drying;
2) TiCl is got according to volume ratio 1:4:60 4solution, 30%H 2o 2, absolute ethyl alcohol, ice-water bath condition lower magnetic force stir, in absolute ethyl alcohol, dropwise drip TiCl 4solution.After solution-stabilized, in solution, dropwise drip 30%H 2o 2, be configured to 195ml colloidal sol and remove ice-water bath after stable, stir 60min, ageing 12h with rotating speed 500r/min;
3) in step 2) basis on, by step 1) ACF that obtains is cut into 4cm*5cm, be connected with power cathode.Positive source links with platinum electrode, together immerses above-mentioned ACF and platinum electrode according to step 2) fixing in the colloidal sol prepared, keep NACF and platinum electrode distance 3cm, voltage 8v, make to remain on 22mA/cm by the current density of NACF 2, electrochemical treatments 80min;
4) in step 3) basis on, by step 3) be put in vacuum tube furnace after the ACF natural drying that obtains, heat treatment 100min under the condition of 400 DEG C, Temperature fall is to room temperature.
With the TiO of gained of the present invention 2/ ACF photocatalysis film material 2cm*2cm small pieces are in 4.5L lucite material Formaldehyde Test case, use type formaldehyde tester, carry out Degradation Formaldehyde test in a hour, test result one hour degradation rate reaches 82.16%, proves that gained thin-film material photocatalysis performance of the present invention is excellent.
Embodiment 5
TiO 2/ NACF nano composite photocatalytic material, adopts following electrochemical preparation method, comprises the following steps:
1) by deionized water, ACF is washed, immerse 24h in salpeter solution.After again washing by deionized water, put into 60 DEG C of oven for drying;
2) TiCl is got according to volume ratio 1:4:60 4solution, 30%H 2o 2, absolute ethyl alcohol, ice-water bath condition lower magnetic force stir, in absolute ethyl alcohol, dropwise drip TiCl 4solution.After solution-stabilized, in solution, dropwise drip 30%H 2o 2, be configured to 260ml colloidal sol, after stable, remove ice-water bath, stir 60min, ageing 12h with rotating speed 500r/min;
3) in step 2) basis on, by step 1) ACF that obtains is cut into 7cm*7cm, be connected with power cathode.Positive source links with platinum electrode, together immerses above-mentioned ACF and platinum electrode according to step 2) fixing in the colloidal sol prepared, keep NACF and platinum electrode distance 3.8cm, voltage 8.6v, make to remain on 27mA/cm by the current density of NACF 2, electrochemical treatments 80min;
4) in step 3) basis on, by step 3) be put in vacuum tube furnace after the ACF natural drying that obtains, heat treatment 100min under the condition of 400 DEG C, Temperature fall is to room temperature.
With the TiO of gained of the present invention 2/ ACF photocatalysis film material 2cm*2cm small pieces are in 4.5L lucite material Formaldehyde Test case, use type formaldehyde tester, carry out Degradation Formaldehyde test in a hour, test result one hour degradation rate reaches 88.31%, proves that gained thin-film material photocatalysis performance of the present invention is excellent.

Claims (9)

1.TiO 2/ NACF nano composite photocatalytic film, it is that on NACF, load has TiO 2film, described TiO 2the thickness of film is 10 ~ 100nm, is following preparation method's products therefrom, comprises the following steps:
1) deionized water detergent active Carbon fibe, soaks 18 ~ 36h in salpeter solution, after again washing, dries by deionized water;
2) by step 1) NACF is cut into suitable size after the process that obtains, be connected with power cathode; Positive source is connected with platinum electrode, NACF and platinum electrode is together immersed in peroxo titanic acid sol fixing, and energising process 40min ~ 80min, obtains TiO 2/ NACF nano thin-film presoma;
3) by step 2) TiO that obtains 2be put in vacuum tube furnace after the natural drying of/NACF nano thin-film presoma, heat treatment 60 ~ 120min under the condition of 150 DEG C ~ 400 DEG C, is down to room temperature naturally.
2. TiO according to claim 1 2/ NACF nano composite photocatalytic film, is characterized in that the preparation method of described peroxo titanic acid sol is: according to volume ratio 1:4:(50 ~ 80) measure TiCl 4solution, H 2o 2and absolute ethyl alcohol, ice-water bath dropwise drips TiCl while stirring in absolute ethyl alcohol 4solution, after solution-stabilized, dropwise drips H in solution 2o 2, after stable, remove ice-water bath, stir 40min ~ 60min, ageing, obtains stable red colloidal sol.
3. TiO according to claim 1 2/ NACF nano composite photocatalytic film, is characterized in that step 1) NACF that uses is commercially available viscose-based active carbon fiber, specific area is 1300 ~ 1500m 2/ g.
4. TiO according to claim 1 2/ NACF nano composite photocatalytic film, is characterized in that step 2) in NACF and platinum electrode to keep at a distance 1cm ~ 5cm, supply voltage 3v ~ 10v, make to remain on 15-25mA/cm by the current density of NACF 2.
5. TiO according to claim 1 2the preparation method of/NACF nano composite photocatalytic film, comprises the following steps:
1) deionized water detergent active Carbon fibe, soaks 18 ~ 36h in salpeter solution, after again washing, dries by deionized water;
2) by step 1) NACF is cut into suitable size after the process that obtains, be connected with power cathode; Positive source is connected with platinum electrode, NACF and platinum electrode is together immersed in peroxo titanic acid sol fixing, and energising process 40min ~ 80min, obtains TiO 2/ NACF nano thin-film presoma;
3) by step 2) TiO that obtains 2be put in vacuum tube furnace after the natural drying of/NACF nano thin-film presoma, heat treatment 60 ~ 120min under the condition of 50 DEG C ~ 400 DEG C, is down to room temperature naturally.
6. TiO according to claim 5 2the preparation method of/NACF nano composite photocatalytic film, is characterized in that the preparation method of described peroxo titanic acid sol is: according to volume ratio 1:4:(50 ~ 80) measure TiCl 4solution, H 2o 2and absolute ethyl alcohol, ice-water bath dropwise drips TiCl while stirring in absolute ethyl alcohol 4solution, after solution-stabilized, dropwise drips H in solution 2o 2, after stable, remove ice-water bath, stir 40min ~ 60min, ageing, obtains stable red colloidal sol.
7. TiO according to claim 5 2the preparation method of/NACF nano composite photocatalytic film, is characterized in that step 1) NACF that uses is commercially available viscose-based active carbon fiber, specific area is 1300 ~ 1500m 2/ g.
8. the TiO according to patent requirements 5 2the preparation method of/NACF nano composite photocatalytic film, is characterized in that step 2) in NACF and platinum electrode to keep at a distance 1cm ~ 5cm, supply voltage 3v ~ 10v, make to remain on 15-25mA/cm by the current density of NACF 2.
9. TiO according to claim 1 2/ NACF nano composite photocatalytic film is as the application of photocatalytic degradation material.
CN201510130664.4A 2015-03-24 2015-03-24 TiO2/activated carbon fiber nano-composite photocatalysis film and preparation method and application thereof Pending CN104689789A (en)

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Publication number Priority date Publication date Assignee Title
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Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2005060877A (en) * 2003-08-11 2005-03-10 Japan Science & Technology Agency Method for producing mesoporous activated carbon fiber
CN1943852A (en) * 2006-10-13 2007-04-11 中国石油大学(华东) Active carbon fiber loaded titanium diotide film optic catalyst and its preparing method and using method
CN101011654A (en) * 2007-01-29 2007-08-08 中国石油大学(华东) Preparing method of activated carbon fibre loading titanium oxide thin film and application method thereof

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Application publication date: 20150610